高效液相色谱-电喷雾电离三级四极杆质谱检测动物源食品中氯霉素、甲砜霉素、氟苯尼考残留量

建立了动物源产品中氯霉素、甲砜霉素、氟苯尼考残留量的高效液相色谱-电喷雾电离三级四极杆质谱(LC-ESI-MS/MS)的方法。前处理方法包括添加同位素内标氯霉素-d5,碱化乙酸乙酯提取,C18小柱净化。该方法采用负离子,多反应监测氯霉素四对离子(321.0/151.9,321.0/256.6,321.0/194.2,321.0/175.4),甲砜霉素两对离子(354.1/185.0,354.1/290.0),氟苯尼考两对离子(356.0/335.9,356.0/185.1)和同位素内标氯霉素-d5(326.0/157.1)。该方法线性范围为0.1~1.6μg/kg;对不同基质样品的加标回收率为80%~112.5%;相对标准偏差小于11%;方法的测定低限为0.1μg/kg。     

带时间窗的三维装载物流配送优化方法研究

针对城市物流配送优化研究在客户服务时间窗和货物装载方式合理结合方面存在的不足,考虑物流配送车厢货物装载方式与客户访问序列相关的特征对车厢空间进行合理的区域划分。首先,构建了包含配送中心的固定成本、配送车辆的运输成本、维修成本、租赁成本和违反时间窗惩罚成本的物流运营成本最小化和配送车辆空间利用率最大化的双目标优化模型;然后,提出一种结合遗传算法(GA)全局搜索能力和禁忌搜索算法(TS)局部搜索能力的GA-TS混合算法求解模型;最后,结合重庆市某配送中心的三维装载物流配送实例数据进行了优化计算,实验结果给出了带时间窗的三维装载物流配送路径优化方案,并进行了不同车厢空间分区模式下平均装载率、物流运营成本和车辆使用数的比较分析。研究表明,当客户需求货物种类数与车辆的空间区域划分数相等且按货物类型进行区域划分时,物流运营成本最小,配送车辆使用数最少和车辆平均装载率最高。     

On line trace enrichment for isolation of vitamin B2 in food samples

Summary Vitamin B₂ was enriched by liquid-solid extraction from large volumes of aqueous samples on a short precolumn. The enriched compounds were transferred onto an analytical reversed-phase column and separated by ion-pair chromatography. The equipment used provides the possibility of automation for routine analysis.Dedicated to Professor J. F. K. Huber on the occasion of the 60th birthday.     

Determination of triclosan in foodstuffs

A reverse-phase high-performance liquid chromatographic (RP-HPLC) method coupled with an ultraviolet detector was developed to determine triclosan which had migrated into foodstuffs from packaging materials. The method includes extraction with hexane, followed by evaporation to dryness and residue re-dissolution in ACN 90%. Chromatographic separation was performed with a Kromasil 100 C18 column (15 cm x 0.4 cm ID, 5 microm particle size) at 30 degrees C and using ACN and water as mobile phases. Regarding recoveries, good results (higher than 83% and lower than 112%) were obtained for the three representative food matrixes selected (orange juice, chicken breast meat, and Gouda cheese).     

富锌排铅咀嚼片安全性毒理学评价

对富锌排铅咀嚼片(RZLR)进行了急性毒性试验、Ames试验、骨髓微核试验、精子畸形试验和30 d喂养试验。结果表明,小鼠急性毒性LD50(BW)>21 500 mg/kg,属无毒级;Ames试验、小鼠骨髓微核试验、精子畸形试验和30 d喂养试验结果均为阴性;30 d喂养试验也未显示明显毒性。本研究证实RZLR是一种安全、无毒副作用的保健食品。     

Thermal analysis,state transitions and food quality

Thermal properties of food systems are important in understanding relationships between food properties and changes in food quality. Concentrated food systems (low-moisture and frozen foods) are seldom in an equilibrium state and they tend to form amorphous, non-crystalline structures. Several glass transition-related changes in such foods affect stability, e.g., stickiness and caking of powders, crispness of snack foods and breakfast cereals, crystallisation of amorphous sugars, recrystallisation of gelatinised starch, ice formation and recrystallisation in frozen foods and rates of non-enzymatic browning and enzymatic reactions. Relationships between glass transition, water plasticisation and relaxation times can be shown in state diagrams. State diagrams are useful as stability or quality maps and in the control of rates of changes in food processing and storage.This revised version was published online in November 2005 with corrections to the Cover Date.     

Do proficiency tests always verify laboratories’ performance? The case of FAPAS PT 0270

In this paper, the case of FAPAS PT 0270 “Doramectin and Oxfendazole in Sheep Liver” is discussed. During evaluation of the data received from participants (determination of total, oxidised oxfendazole residue and calculation of the sum of oxfendazole and oxfendazole sulfone residues), significant differences were observed between the results obtained by use of two analytical approaches. This phenomenon can be explained by the route of oxfendazole metabolism, which results in the presence of fenbendazole in the sample. This was not predicted by the provider; consequently, not all the necessary tests on the material were conducted. Due to the high uncertainty of the z-scores in this test, the results of the PT cannot be used for purposes of evaluation, and the benefits of participation in PT 0270 are questionable.     

固体超强酸SO_4~(2-)/SiO_2-TiO_2催化合成异维生素C钠

在异维生素C钠(D-VcNa)的合成过程中,以SO42-/S iO2-TiO2复合固体超强酸作为酯化反应催化剂,2-酮基-D-葡萄糖酸(2-KGA)和甲醇为原料,采用精馏脱水酯化工艺,不断除去酯化过程中产生的水。催化剂的最佳焙烧温度为550℃,催化剂用量为2.5%;反应时间3~4 h,产品收率为88.6%,催化剂的重复使用性较好,催化体系优于硫酸法。     

Application of differential scanning calorimetry in food research and food quality assurance

Differential scanning calorimetry (DSC) is the most widely used thermal analytical technique in food research and it has a great utility in quality assurance of food. Proteins are the most studied food components by thermal analysis including studies on conformation changes of food proteins as affected by various environmental factors, thermal denaturation of tissue proteins, food enzymes and enzyme preparations for the food industry, as well as effects of various additives on their thermal properties. Freezing-induced denaturation of food proteins and the effect of cryoprotectants are also monitored by DSC. Polymer characterization based on DSC of polysaccharides, gelatinization behaviour of starches and interaction of starch with other food components can be determined, and phase transitions during baking processes can be studied by DSC. Studies on crystallization and melting behaviour of fats observed by DSC indicate changes in lipid composition or help characterizing products. Thermal oxidative decomposition of edible oils examined by DSC can be used for predicting oil stability. Using DSC in the freezing range has a great potential for measuring and modelling frozen food thermal properties, and to estimate the state of water in foods and food ingredients. Research in food microbiology utilizes DSC in better understanding thermoadaptive mechanisms or heat killing of food-borne microorganisms. Isothermic microcalorimetric techniques provide informative data regarding microbial growth and microbial metabolism.     

Simultaneous screening and determination eight phthalates in plastic products for food use by sonication-assisted extraction/GC-MS methods

Studies on determination of eight kinds of phthalates, e.g. di-ethyl phthalate (DEP), di-propyl phthalate (DPP), di-isobutyl phthalate (DIBP), di-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-cyclohexyl phthalate (DCHP), di-(2-ethylhexyl) phthalate (DEHP), di-octyl phthalate (DOP), in 25 kinds of plastic products for food use, including packaging bags, packaging film, containers, boxes for microwave oven use, sucking tubes, spoons, cups, plates, etc. by gas chromatography in combination with mass spectrometry detector (GC-MS) in electronic ionisation mode (EI) with selected-ion monitoring (SIM) acquisition method (GC-MS (EI-SIM)) have been carried out. Methods have been developed for both qualitative and quantitative analysis of phthalates. Extraction, clean-up and analysis procedure have been optimized. Determination of samples were performed after frozen in liquid nitrogen and sonication-assisted extraction with hexane, clean-up with LC-C18 SPE and analyzed by GC-MS methods. The base peak (m/z = 149) of all the phthalates was selected for the screening studies. The characteristic ions, 121, 177, 222 for DEP; 191, 209 for DPP; 57, 223 for DIBP; 104 for DBP; 91, 132, 206 for BBP; 55, 167 for DCHP; 113, 167, 279 for DEHP; 279 for DOP were chosen for quantitative studies. These techniques are possible to detect phthalates at the level of 10.0 μg/kg. Overall recoveries were 82-106% with R.S.D. values at 3.8-10.2%. Only one of the 25 examined samples was free from phthalates. The rest 24 samples were found to contain at least three or more of these phthalates. The predominant phthalate detected in the studied samples was DEHP.